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DOE OSTI2025

Trace Element Analyses of Micron-Size Particles and Statistical Determination of Minimum Detection Limits

Savannah River National Laboratory (SRNL) has developed expertise in producing homogeneous, ca. 1 m-diameter spherical particles of mixed-element components, wherein dopants can be varied from a trace constituent (ppm) to wt.% concentrations. The samples used for this work are nickel-doped cerium oxide microspheres produced by SRNL. They were initially selected as analogs for plutonium-doped uranium oxide particles and analyzed as part of a larger study to evaluate whether electron probe microanalyzers (EPMA) can be used to characterize nuclear materials as an alternative or complementary method to mass spectrometers. The five samples used in this study contained nominal compositions of 0, 0.004, 0.04, 0.4 and 4 wt.% Ni. They were analyzed by both an Agilent 7900 Q-ICP-MS at SRNL and the JEOL JXA8530F Plus EPMA at the University of Minnesota. In addition to EPMA results (calibrated with high-precision Q-ICP-MS analyses) suggesting that the EPMA could address outstanding nuclear material characterization needs, these samples 1) showcase the ability of the EPMA to quantify not just trace concentrations, but trace concentrations in microparticles (1 m diameter, Fig. 1), and 2) offer a unique opportunity to evaluate the methodology for assessing the minimum detection limits of EPMA analyses.

McSwiggen, Peter [JEOL USA, 11 Dearborn Road, Peab↗

NASA NTRS1980

Pollution Detection Devices

Barringer Research, Inc.'s COSPEC IVB (correlation spectrometer) can sense from a considerable distance emissions from a volcanic eruption. Remote sensor is capable of measuring sulfur dioxide and nitrogen dioxide in the atmosphere. An associated product, GASPEC, a compression of Non-dispersive Gas Filter Spectrometer, is an infrared/ultraviolet gas analyzer which can be used as either a ground based detector or in aircraft/spacecraft applications. Extremely sensitive, it is useful in air pollution investigations for detecting a variety of trace elements, vapors, which exist in the atmosphere in small amounts.

Source record↗

NASA NTRS1989

The measurement of trace elements in interplanetary dust and cometary particles by ultra-high sensitivity INAA

Today the major elemental composition of interplanetary dust particles (IDPs) is routinely determined in many laboratories. These and mineralogical studies have revealed the presence of at least two major types of IDPs, chondritic and refractory. Preliminary results of a successful attempt to determine abundances of a large suite of trace elements from both chondritic and refractory IDPs are reported. The analytical procedure can be used in the grain-by-grain analysis of returned cometary samples. Chondritic and refractory IDPs are characterized by standard scanning electron microscopy and energy dispersive x ray spectroscopy (SEM-EDX) techniques. With this system, detection limits for many elements are well below picogram levels, and some approach femtogram levels. This technique is non-destructive, although some sample handling is required, so particles can be analyzed by other techniques after instrument neutron activation analysis (INAA) is completed. Data is presently being reduced from the analyses of 7 IDPs. These are U2015E10, U2015F1, W7029-A2, W7029-A3, W7013A8, LACl (all chondritic) and 705 (refractory). So far, 17 different major and trace elements were detected and measured in these particles, including rare earths and some very volatile elements (Br and Zn).

Zolensky, M. E.↗

DOE OSTI2025

Abstract for CRADA between NETL and GlycoSurf, Inc.

The National Energy Technology Laboratory (NETL) and GlycoSurf, Inc. (Participant) will collaborate in the development of novel luminescent sensing materials for rare earth elements using chemically modified surfactants. Rare earth elements are economically critical metals that are used in many technologies relevant to both energy and national defense. Slow and expensive characterization methods for rare earth element analysis are a major pain point for domestic production of these metals; the development of low-cost optical sensing materials and platforms can significantly reduce the time and financial costs associated with rare earth element prospecting and process monitoring. NETL has extensive experience developing inexpensive and compact optical sensors for critical metals such as rare earths. GlycoSurf, Inc. has commercialized high performance surfactants for the selective extraction of rare earth elements in complex environments such as acid mine drainage. By modifying these surfactants with fluorescent functional groups, trace concentrations of rare earths may be detected through a process called “photosensitization,” where the sensing material induces element-specific emission bands that enable different rare earth elements to be detected and distinguished. This project will enable the development of sensing materials capable of selectively detecting trace quantities of valuable rare earths in challenging conditions, including high ionic strength, highly acidic matrices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRSDate not supplied

Mineralogical, Elemental and Tomographic Reconnaissance Investigation for CLPS (“METRIC”)

METRIC comprises a suite of two instruments in a Lunar lander that perform X-ray diffraction (XRD) for mineral structure, X-ray fluorescence (XRF) for elemental composition, and X-ray Micro Computed Tomography (XCT) for 3D internal micromorphology. The instruments are accompanied by optical-near IR cameras to provide local geologic context. The Honeybee Robotics PlanetVac pneumatic sampling and transfer system [1],positioned on a lander footpad, will deliver sieved regolith to the X-ray instruments for analysis. The instrument suite is intended for delivery to the lunar surface on a Commercial Lunar Payload Services (CLPS) lander. The METRICXRD/F instrument draws on heritage from the Mars Science Laboratory CheMin instrument [2] and improves upon the design in multiple ways [3]. Like CheMin, Rietveld refinement and full-pattern fitting of METRIC XRD data can identify minerals at a detection limit of ~1 wt.%, quantify their abundances when present at >3 wt.%, and determine mineral composition (e.g., Fo#in olivine) from lattice parameters for minerals present at >5 wt.%[4,5]. An optimized XRF geometry provides for improved detection and quantification of major, minor and trace elements. The METRIC XCT instrument is a miniaturized X-ray Computed Tomography scanner[6]. Lunar regolith is delivered to a 3 mm diameter, 10 mm long graphite tube inside the instrument. The tube is rotated through 360°in 0.9deg.incrementsand a divergent point source X-ray beam is directed through the material. A Charge Coupled Device (CCD)records attenuation images whose brightness and contrast area function of average atomic number and density. Quantitative data, including particle and void sizes, 3D particle shape parameters, modal volumes and pore geometry can be derived from the resulting 3D reconstructions(voxel resolution: 30 μm). Crystal morphologies derived from METRIC XCT data complement the bulk mineralogy determined by the METRIC XRD/F and provide a measure of grain size distribution for the different phases. Taken together, the METRIC instrument suite determines crystal structure, elemental composition and morphology, three principal characteristics of geological materials that are highly useful in determining the origin and subsequent processing of lunar regolith.

Moon↗

NASA NTRS2012

Design for the Structure and the Mechanics of Moballs

The moball is envisioned to be a round, self-powered, and wind-driven multifunctioning sensor used in the Gone with the Wind ON-Mars (GOWON) [http://www.lpi.usra.edu/meetings/ marsconcepts2012/pdf/4238.pdf]: A Wind-Driven Networked System of Mobile sensors on Mars. The moballs would have sensing, processing, and communication capabilities. The moballs would perform in situ detection of key environmental elements such as vaporized water, trace gases, wind, dust, clouds, light and UV exposure, temperature, as well as minerals of interest, possible biosignatures, surface magnetic and electric fields, etc. The embedded various low-power micro instruments could include a Multispectral Microscopic Imager (to detect various minerals), a compact curved focal plane array camera (UV/Vis/NIR) with a large field of view, a compact UV/Visible spectrometer, a micro-weather station, etc. The moballs could communicate with each other and an orbiter. Their wind- or gravity-driven rolling movement could be used to harvest and store electric energy. They could also generate and store energy using the sunlight, when available, and the diurnal temperature variations on Mars. The moballs would be self-aware of their (and their neighbors ) positions, energy storage, and memory availability; they would have processing power and could intelligently cooperate with neighboring moballs by distributing tasks, sharing data, and fusing information. The major advantages of using the wind-driven and spherical moball network over rovers or other fixed sensor webs to explore Mars would be: (1) moballs could explore a much larger expanse of Mars in a much faster fashion, (2) they could explore the difficult terrains such as steep slopes and sand dunes, and (3) they would be self-energy- generating and could work together and move around autonomously. The challenge in designing the structure and the mechanics of the moball would be that it should be sturdy enough to withstand the impact of its initial fall, as well as other impacts from obstacles in its way. A mechanism would be needed that could enable hundreds of moballs to be carried while they would be deflated and compact, then would inflate them just after deploying them to their drop site. Furthermore, the moballs should also be light enough to allow them to move easily over obstacles by force of the wind. They also should have some kind of maneuvering mechanism in place to help them avoid very hazardous sharp objects or events, and to enable them to get closer to the objects of interest. The structure of the moballs was designed so that they would have different layers. The outer layer should comprise a sturdy, yet light, polymer that could withstand both the impact of the initial drop, as well as the impact of the different obstacles it would encounter while traversing the surface of Mars. This polymer should not deteriorate with the 100 K daily temperature swings on Mars. The inner layer should consist of a very light gas such as nitrogen or helium. In terms of maneuvering, six very light weights placed at strategic locations would give moballs the ability to turn, or even hop, over hazardous (e.g., sharp) obstacles, or even initiate a movement (before getting more help from the wind to be carried around) when stuck. Maneuvering would be necessary in order to get closer to objects of interest. If the weights would be allowed to move freely, they could also be used to generate energy.

Davoodi, Faranak↗

NASA NTRS1978

Lonar crater glasses and high-magnesium australites - Trace element volatilization and meteoritic contamination

Radiochemical neutron activation analysis was used to detect six siderophile elements (Ni, Re, Os, Pd, Ir and Au) and three volatile elements (Zn, Se and Cd) in two basalts, a pumice and three impact glasses from Lonar crater, India, and in six high-magnesium australites. Significant depletions in Re and Se with respect to the parent basalts were found in the Lonar glasses. These depletions, apparently correlated with the degree of shock, are probably due to volatilization under the oxidizing conditions characteristic of earth. One of the australites is substantially enriched in siderophiles relative to the level of these elements in the other five tektites. The element patterns in the australites resemble those of the carbonaceous or cometary component of an Apollo 16 soil.

Morgan, J. W.↗

DOE OSTI2016

Imaging trace element distributions in single organelles and subcellular features

The distributions of chemical elements within cells are of prime importance in a wide range of basic and applied biochemical research. An example is the role of the subcellular Zn distribution in Zn homeostasis in insulin producing pancreatic beta cells and the development of type 2 diabetes mellitus. We combined transmission electron microscopy with micro- and nano-synchrotron X-ray fluorescence to image unequivocally for the first time, to the best of our knowledge, the natural elemental distributions, including those of trace elements, in single organelles and other subcellular features. Detected elements include Cl, K, Ca, Co, Ni, Cu, Zn and Cd (which some cells were supplemented with). Cell samples were prepared by a technique that minimally affects the natural elemental concentrations and distributions, and without using fluorescent indicators.We find it could likely be applied to all cell types and provide new biochemical insights at the single organelle level not available from organelle population level studies.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2026

Advanced Characterization of Wastewaters with a Focus on the Environment & Economics (Final Technical Progress Report)

This project, funded by the U.S. Department of Energy under award DE-FE0032457 and conducted at the University of Illinois at Urbana-Champaign, focused on advancing the characterization of coal combustion residual (CCR) effluents. The primary objectives were to develop analytical methods for detecting major cations, anions, trace metals, and rare earth elements (REEs) in CCR wastewater, assess environmental impacts, and explore opportunities for resource recovery. The project advanced the development of a "One-Shot" analysis system designed to simultaneously analyze multiple analytes in CCR effluents.

01 COAL, LIGNITE, AND PEAT↗

NASA NTRS1976

Inorganic analyses of Martian surface samples at the Viking landing sites

Elemental analyses of fines in the Martian regolith at two widely separated landing sites, Chryse Planitia and Utopia Planitia, produced remarkably similar results. At both sites, the uppermost regolith contains abundant Si and Fe, with significant concentrations of Mg, Al, S, Ca, and Ti. The S concentration is one to two orders of magnitude higher, and K (less than 0.25% by weight) is at least 5 times lower than the average for earth's crust. The trace elements Sr, Y, and possibly Zr have been detected at concentrations near or below 100 parts per million. Pebble-sized fragments sampled at Chryse contain more S than the bulk fines and are thought to be pieces of a sulfate-cemented duricrust.

Clark, B. C.↗

DOE OSTI2025

Low-cost, portable optical sensors for critical mineral prospecting and process monitoring

A combination of projected demand increases for economically critical minerals and a monopolistic global marketplace for these minerals has caused concern over supply chain vulnerabilities, which would impact energy, national defense, and advanced technology production. Domestic production of critical minerals is hindered by expensive and non-portable methods for analyzing metal concentration, which is vital both for resource prospecting and process monitoring. Here, a suite of luminescent materials along with portable instrumentation is presented for fluorescence-based detection of trace concentrations of critical minerals (cobalt, rare earth elements, and aluminum) as well as common gangue metals that are removed during processing (iron and aluminum). A metal-organic framework comprised of zinc, adenine, and trimesic acid immobilized on a fiber optic tip is capable of sensing part-per-billion concentrations of terbium, europium, dysprosium, and samarium through a sensitization approach, in which individual elements produce characteristic emission bands enabling multiple rare earths to be simultaneously detected and distinguished. A deep-UV light emitting diode is used as the excitation source, while a portable spectrometer is used to detect the emitted light. A similar optical set-up is coupled with two different carbon dot materials, which can detect low part-per-million concentrations of cobalt and iron in acidic environments. Metal-organic framework thin films comprised of copper and 2-aminoterephthalic acid are used in tandem with a portable optical set-up to further detect aluminum, with successful deployment in real fly ash leachates. Taken together, these technologies provide an inexpensive and sensitive path towards characterizing economically critical metals.

characterization and extraction of rare earth elem↗

DOE OSTI2019

Ambient vapor sampling and selective cluster formation for the trace detection of tributyl phosphate via atmospheric flow tube mass spectrometry

In addition to serving as an f-element ligand and rare-earth method complexing agent, tributyl phosphate (TBP) is a compound containing core functional groups that mimic those routinely found in degradation products from industrial processes. Because detection of trace quantities of TBP can provide insight into the routes of contamination and degradation in the environment, there is a need to develop methods capable of detecting trace quantities of TBP. Vapor detection at atmospheric pressure is one approach that is both sensitive and rapid. We present here the use of atmospheric flow tube mass spectrometry (AFT-MS) for the ambient vapor sampling of TBP from headspace of ppb-level solutions in methanol. Gas phase clustering reactions were to enhance detection levels via the addition of small quantities of the dopants diethylamine (DEA), triethylamine (TEA), and pinacolyl methylphosphonate (PMP) in the vapor stream. Detection of the TBP vapor emanating from these solutions demonstrated a linear range for the protonated TBP species of 1-1000 ppb from solution. The clusters of TBP with DEA, TEA, and PMP each yielded linear ranges of 1-250 ppb for TBP in solution. Despite smaller linear ranges, the addition of these dopant species added a layer of analytical selectivity and reduced variability in signals from quality control samples. These data were obtained using an AFT source coupled to a linear ion trap mass spectrometer, which demonstrates the applicability of trapping systems to the AFT ionization technique while monitoring positive ions.

Ambient vapor sampling, Dielectric barrier dischar↗

DOE OSTI2016

Elemental analysis of different varieties of rice samples using XRF technique

Rice is most consumed staple food in the world providing over 21% of the calorie intake of world’s population having high yielding capacity. Elements detected in rice are Al, As, Br, Cd, Cl, Co, Cs, Cu, Fe, Hg, K, Mg, Mn, Mo, Rb, Se and Zn by using Instrumental Neutron Activation with k0 standardization (R. Jayasekera etal,2004). Some of these trace elements are C, H, O, N, S, Ca, P, K, Na, Cl, Mn, Ti, Mg, Cu, Fe, Ni, Si and Zn are essential for growth of human physique The deficiency or excess of these elements in food is known to cause a variety of malnutrition or health disorders in the world. Every year, various varieties of rice are launched by Punjab Agriculture University, Ludhiana. The main purpose of which is to increases the yield to attain the maximum profit. But this leads to changing the elemental concentration in them, which may affect the human health according to variation in the nutrition values. The main objective is to study the presence of elemental concentration in various varieties of rice using EDXRF technique.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2019

Methylmercury Speciation and Retention Evaluation to Support Saltstone Waste Acceptance Criteria

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS1975

Volatiles on the surface of Apollo 15 green glass and trace-element distributions among Apollo 15 soils

Zn, Ge, Cd, In, and Au have been detected in surficial deposits on Apollo 15 green-glass spherules, and it is suggested that these deposits are condensates from the magmatic gas phase which was responsible for the pneumatic expulsion of the green glass from the lunar interior. Thermodynamic data indicate that chlorides and fluorides were the dominant forms of the volatile metals. The Ar-40x content of a nongreen-glass soil fraction is greater than that found in green-glass. Mare and low-K Fra Mauro basalts seem to be the most prominent components of Apollo 15 soil. The correlation of Zn with Ar-40x and with Pb-204 is studied, and the distribution of quartz-normative and olivine-normative basalts is considered.

Chou, C.-L.↗

DOE OSTI2025

Detection and quantification of trace technetium in the presence of molybdenum using laser-induced breakdown spectroscopy

Technetium (Tc) is a very important element that is encountered in many aspects, from its presence in radioactive waste and its potential environmental impact to its use as a medical radioisotope. Its detection and quantification in liquid samples is traditionally cumbersome, involving detailed sample preparation and analysis by mass spectrometry or scintillation. This article demonstrates the first comprehensive emission spectral analysis of Tc from a liquid sample by immobilization in a polymer and analysis by laser-induced breakdown spectroscopy (LIBS). A survey of LIBS spectra was completed to identify the strongest analytical lines for quantification of trace Tc in the presence of Mo. The quantification of Tc in a Mo-containing matrix was selected because Tc radioisotopes are the daughter products of Mo isotope decay. The first reported calibration curves by LIBS are provided with limits of detection and quantification down to 0.710 µg mL −1 and 1.39 µg mL −1 , respectively. Ultimately, this study demonstrated the feasibility of trace Tc quantification using LIBS and will serve as a reference for future research related to monitoring this radioactive species.

Andrews, Hunter B. [Oak Ridge National Laboratory ↗

DOE OSTI2015

Nanosecond Nd-YAG laser induced plasma emission characteristics in low pressure CO{sub 2} ambient gas for spectrochemical application on Mars

An experimental study is conducted on the possibility and viability of performing spectrochemical analysis of carbon and other elements in trace amount in Mars, in particular, the clean detection of C, which is indispensible for tracking the sign of life in Mars. For this study, a nanosecond Nd-YAG laser is employed to generate plasma emission from a pure copper target in CO{sub 2} ambient gas of reduced pressure simulating the atmospheric condition of Mars. It is shown that the same shock wave excitation mechanism also works this case while exhibiting remarkably long cooling stage. The highest Cu emission intensities induced by 4 mJ laser ablation energy is attained in 600 Pa CO{sub 2} ambient gas. Meanwhile the considerably weaker carbon emission from the CO{sub 2} gas appears relatively featureless over the entire range of pressure variation, posing a serious problem for sensitive trace analysis of C contained in a solid sample. Our time resolved intensity measurement nevertheless reveals earlier appearance of C emission from the CO{sub 2} gas with a limited duration from 50 ns to 400 ns after the laser irradiation, well before the initial appearance of the long lasting C emission from the solid target at about 1 μs, due to the different C-releasing processes from their different host materials. The unwanted C emission from the ambient gas can thus be eliminated from the detected spectrum by a proper time gated detection window. The excellent spectra of carbon, aluminum, calcium, sodium, hydrogen, and oxygen obtained from an agate sample are presented to further demonstrate and verify merit of this special time gated LIBS using CO{sub 2} ambient gas and suggesting its viability for broad ranging in-situ applications in Mars.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2019

Mercury Speciation and Stabilization in Saltstone - 19103

Mercury is a contaminant of concern in Savannah River Site (SRS) high level waste (HLW). For five decades elemental mercury was used in the catalytic dissolution of aluminum cladding from the enriched-alloy uranium recovery process. Over 60,000 kg of mercury are now distributed in the SRS HLW tanks. The mercury speciation in the liquid waste streams resulting from conditioning HLW sludge for vitrification and in the decontaminated low activity sodium salt solution removed from the tanks was initially thought to be primarily ionic with a minor amount of elemental mercury. Recent sampling detected organic mercury, primarily methylmercury, HgCH{sub 3}{sup +} (MeHg{sup +}), and a trace amount of ethylmercury (EtHg) in these streams in addition to the ionic and elemental forms of mercury. The objective of this work was to identify the fate of the organic mercury in saltstone, a waste form containing portland cement, slag cement, and Class F fly ash. This information is needed to evaluate total mercury and organic mercury limits for the saltstone Waste Acceptance Criteria to assure regulatory compliance with mixed waste disposal requirements and to evaluate opportunities to enhance the waste form performance. Results to date indicate that the MeHg{sup +} reacts with sulfide in the cementitious reagents, slag in particular, to form nanoparticles of β-HgS, meta cinnabar, which is very insoluble and has a solubility product in water, pK{sub sp}, at 25 deg. C of 53. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗